CN108365175A - A kind of mixed network structure of three-dimensional interconnection, Preparation method and use - Google Patents

A kind of mixed network structure of three-dimensional interconnection, Preparation method and use Download PDF

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CN108365175A
CN108365175A CN201810128640.9A CN201810128640A CN108365175A CN 108365175 A CN108365175 A CN 108365175A CN 201810128640 A CN201810128640 A CN 201810128640A CN 108365175 A CN108365175 A CN 108365175A
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network structure
preparation
mixed
dimensional
mixed network
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龙剑平
胡安俊
舒朝著
梁冉曦
李嘉宝
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Chengdu Univeristy of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a kind of preparation methods of the mixed network structure of three-dimensional interconnection, and carbon nanotube/neopelex mixed solution, sodium molybdate and thiocarbamide is filtered, washed after hydro-thermal reaction, is dried, the wherein surface functionalized processing of carbon nanotube.The present invention will be incorporated by the carbon nanotube of surface functionalization in molybdenum disulfide nano sheet stepped construction, improve the electron conduction of molybdenum disulfide, molybdenum disulfide nano sheet stacking can also be reduced, is formed and detaches good three-dimensional meso-hole nano hybridization network so that active surface area dramatically increases.And due to unique three-dimensional meso-hole nanostructure so that molybdenum disulfide/carbon mano-tube composite provides excellent chemical property in terms of specific capacity, high rate performance and long-term cycle stability.

Description

A kind of mixed network structure of three-dimensional interconnection, Preparation method and use
Technical field
The present invention relates to electrode fields, and in particular to a kind of mixed network structure of three-dimensional interconnection, Preparation method and use.
Background technology
Due to the global warming of non-renewable fossil fuel consumed excessively with getting worse, green is greatly developed and can Continuous energy (such as wind energy, solar energy, tide energy) is of great significance.Secondary cell is a kind of promising electrochemical storage System directly can convert chemical energy to electric energy by reversible electrochemical redox reaction.Wherein, lithium ion battery (lithium-ionbatteries, LIBs) is current most popular and most efficient energy-storage system, and it is potential almost to realize its Maximum performance (i.e. energy density 250Whkg-1), however low energy density limits it is needing high energy battery system It is widely used, such as battery powered electric vehicle (electric vehicles, EVs).In various battery systems being developed In, the highest theoretical energy density of lithium-aeration cell (lithium-air battery, LABs) is about 3608Whkg-1It (is based on Reversible reactionE °=2.96V), it is considered to be one of most promising next generation's battery technology.
Although there is LABs vast potential for future development, many science and technology limitations to hinder its further development, packet Include the technological challenges such as the cyclical stability of low energy efficiency, the high rate performance of difference and difference.To overcome the problems, such as these, do Many effort are gone out, wherein most simple and effective solution is to promote the catalytic activity of electrode material using catalyst.Perhaps Multi-catalyst (such as carbon material, metal oxide, carbonitride and noble metal) has been used as the cathod catalyst of LABs, with Just overpotential is reduced, promotes reaction process, and inhibit the decomposition of electrolyte.
Recently, it is inspired by grapheme material immense success, two-dimentional molybdenum disulfide (MoS2) in different electrochemistry It is explored in system, including Hydrogen evolving reaction, carbon dioxide conversion and ORR, due to its excellent catalytic activity.Especially exist The fields LABs, to MoS2Some important researchs are carried out.However, MoS2Electric conductivity it is poor, and carbon material combination It is to overcome MoS2The available strategy of this disadvantage and optimization performance.
Invention content
The purpose of the present invention is to provide a kind of preparation method of the mixed network structure of three-dimensional interconnection, this method passes through one Footwork is synthesized by ultra-thin stratiform MoS2Sheetlike material (the MoS of nanometer sheet and high conductivity CNT compositions2/CNTs).The knot of CNT The electron conduction of nano hybrid can not only be improved by closing, but also can reduce MoS2Nanometer sheet is laminated, and it is good to form separation Ultrathin membrane, lead to the significant increase of active surface area.In addition, the ultra-thin MoS with high surface area2Nanometer sheet can promote ion With the fast transportation of electronics.Benefit from above-mentioned unique 3D structures, MoS2/ CNT nano-mixtures in specific capacity, high rate performance and Remarkable chemical property is provided in terms of long-term cycle stability.Such a unique solution manufactures for actual industrial Provide high rate capability, simple, inexpensive and expansible MoS2The powerful way of the rational design of/CNT cathode materials.
The present invention is achieved through the following technical solutions：
A kind of preparation method of the mixed network structure of three-dimensional interconnection mixes carbon nanotube/neopelex Solution, sodium molybdate and thiocarbamide are filtered, washed after hydro-thermal reaction, dry, the wherein surface functionalized processing of carbon nanotube.
The surface functionalization of carbon nanotube is ultrasonically treated specifically, carbon nanotube is added in sulfuric acid and nitric acid mixed solution Afterwards, heat, filter, washing, be dried in vacuum overnight after obtain the carbon nanotube of surface functionalization.
It is ultrasonically treated 10~15min.
It is heated to be 60~80 DEG C of 1~2h of oil bath heating.
Vacuum drying is 50~60 DEG C.
Carbon nanotube/neopelex mixed solution, sodium molybdate and thiocarbamide need to be add to deionized water progress It is ultrasonically treated 30~35min.
Carbon nanotube/neopelex mixed solution is that 200mg carbon nanotubes are dispersed in 1000ml dodecanes In base benzene sulfonic acid sodium salt, it is ultrasonically treated 1~1.5h.
Mass ratio between carbon nanotube and sodium molybdate, thiocarbamide is 4:151:200.Carbon nano-tube solution in preparation process The too small MoS for being not easy to isolating plate-like of volume2, crossing conference leads to MoS2Disperse uneven, lamella is not of uniform size.Sodium molybdate and The molar ratio of thiocarbamide is to MoS2Piece thickness has an impact.
The mixed network structure for the three-dimensional interconnection that foregoing preparation method obtains is three-dimensional meso-hole nanometer network knot Structure.
The mixed network structure of foregoing three-dimensional interconnection, in the application as lithium air electrode material.
Compared with prior art, the present invention having the following advantages and advantages：
The present invention will be incorporated by the carbon nanotube of surface functionalization in molybdenum disulfide nano sheet stepped construction, be improved The electron conduction of molybdenum disulfide, additionally it is possible to reduce molybdenum disulfide nano sheet stacking, be formed and detach good three-dimensional meso-hole nanometer Hybridization network so that active surface area dramatically increases.And due to unique three-dimensional meso-hole nanostructure so that molybdenum disulfide/carbon Nanotube complex provides excellent chemical property in terms of specific capacity, high rate performance and long-term cycle stability.
Performance of the mixed network structure for the three-dimensional interconnection that the present invention is prepared as lithium air electrode material：1) for the first time Charge-discharge performance：With MoS2The lithium-air battery of/CNTs cathodes provides~6200mAh/g under the current density of 200mA/g Discharge capacity, be charged and discharged overpotential down to 1.06V and 0.34V, promote the energy efficiency of battery.2) high rate performance：Tool There is MoS2The lithium-air battery of/CNTs cathodes under the current density of 100-500mA/g, has good high rate performance respectively, Charging/discharging voltage has almost no change.3) cycle performance：With MoS2Electricity of the lithium-air battery of/CNTs cathodes in 200mA/g Stablize cycle under current density 50 times, cycle performance is good.
Description of the drawings
Attached drawing described herein is used for providing further understanding the embodiment of the present invention, constitutes one of the application Point, do not constitute the restriction to the embodiment of the present invention.In the accompanying drawings：
The mixed network structure SEM figures for the three-dimensional interconnection that Fig. 1 is provided by embodiment 1；
The mixed network structure TEM figures for the three-dimensional interconnection that Fig. 2 is provided by embodiment 1；
The mixed network structure BET figures for the three-dimensional interconnection that Fig. 3 is provided by embodiment 1；
The weightless figure of the mixed network structure for the three-dimensional interconnection that Fig. 4 is provided by embodiment 1；
The combination of the mixed network structure for the three-dimensional interconnection that Fig. 5 is provided by embodiment 1 can be schemed；
The mixed network structure for the three-dimensional interconnection that Fig. 6 is provided by embodiment 1 fills for the first time as lithium air electrode material Electric discharge figure；
The mixed network structure for the three-dimensional interconnection that Fig. 7 is provided by embodiment 1 is as the forthright again of lithium air electrode material It can figure；
Cyclicity of the mixed network structure for the three-dimensional interconnection that Fig. 8 is provided by embodiment 1 as lithium air electrode material It can figure.
Specific implementation mode
To make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiment and attached drawing, to this Invention is described in further detail, and exemplary embodiment of the invention and its explanation are only used for explaining the present invention, do not make For limitation of the invention.
A kind of preparation method of the mixed network structure of three-dimensional interconnection mixes carbon nanotube/neopelex Solution, sodium molybdate and thiocarbamide are filtered, washed after hydro-thermal reaction, dry, the wherein surface functionalized processing of carbon nanotube.
The surface functionalization of carbon nanotube is ultrasonically treated specifically, carbon nanotube is added in sulfuric acid and nitric acid mixed solution Afterwards, heat, filter, washing, be dried in vacuum overnight after obtain the carbon nanotube of surface functionalization.
Embodiment 1
The surface functionalization of carbon nanotube (CNTs)：
80mlH is added in 1gCNTs2SO4And HNO3In mixed solution after ultrasound 10min, in 80 DEG C of oil bath heating 2h, take out Filter, is washed with deionized, and be dried overnight in vacuum drying oven at 60 DEG C, and obtaining that treated, CNTs is for use.
MoS2The synthesis of/CNT：
1) CNTs of 200mg surface functionalization is dispersed in 1000ml neopelexes (SDBS) solution (0.2% W/w in), it is ultrasonically treated 1h, it is spare as carbon source.
2) by 151mg sodium molybdates, 1h is to no obvious sediment for the mixing of 200mg thiocarbamides, then again will be at this solution ultrasound 30min is managed, is subsequently added into 25mlCNTs dispersion liquids and 45ml deionized waters to mixed solution, and continues to be ultrasonically treated 30min.
3) it and then by uniform solution is transferred in reaction kettle, and is heated 24 hours at 220 DEG C.By black suspension mistake It filters and is washed with deionized for several times, it is then dry in vacuum drying oven.Finally obtain MoS2/CNTs。
By the mixed network structure for the three-dimensional interconnection that embodiment 1 obtains, the three-dimensional meso-hole nanometer network of high degree of dispersion is (such as SEM Fig. 1, TEM Fig. 2), the significant increase (such as BET Fig. 3) of active surface area provides a large amount of reactivity site.Its weight loss It can be as shown in Figure 5 as shown in figure 4, combining.1) charge-discharge property：With MoS2The lithium-air battery of/CNTs cathodes exists ~the discharge capacity of 6200mAh/g under the current density of 200mA/g, is provided, be charged and discharged overpotential down to 1.06V and 0.34V promotes the energy efficiency of battery, as shown in Figure 6.2) high rate performance：With MoS2The lithium-air battery of/CNTs cathodes point Not under the current density of 100-500mA/g, there is good high rate performance, charging/discharging voltage has almost no change, such as Fig. 7 institutes Show.3) cycle performance：With MoS2The lithium-air battery of/CNTs cathodes stablizes cycle 50 times under the current density of 200mA/g, Cycle performance is good, as shown in Figure 8.
Embodiment 2
The surface functionalization of carbon nanotube (CNTs)：
80mlH is added in 1gCNTs2SO4And HNO3In mixed solution after ultrasound 10min, in 60 DEG C of oil bath heating 1.5h, take out Filter, is washed with deionized, and be dried overnight in vacuum drying oven at 60 DEG C, and obtaining that treated, CNTs is for use.
MoS2The synthesis of/CNT：
1) CNTs of 200mg surface functionalization is dispersed in 1000ml neopelexes (SDBS) solution (0.2% W/w in), it is ultrasonically treated 1.5h, it is spare as carbon source.
2) by 151mg sodium molybdates, 1h is to no obvious sediment for the mixing of 200mg thiocarbamides, then again will be at this solution ultrasound 30min is managed, is subsequently added into 25mlCNTs dispersion liquids and 45ml deionized waters to mixed solution, and continues to be ultrasonically treated 30min.
3) it and then by uniform solution is transferred in reaction kettle, and is heated 24 hours at 220 DEG C.By black suspension mistake It filters and is washed with deionized for several times, it is then dry in vacuum drying oven.Finally obtain MoS2/CNTs。
Embodiment 3
The surface functionalization of carbon nanotube (CNTs)：
80mlH is added in 1gCNTs2SO4And HNO3In mixed solution after ultrasound 10min, in 80 DEG C of oil bath heating 2h, take out Filter, is washed with deionized, and be dried overnight in vacuum drying oven at 60 DEG C, and obtaining that treated, CNTs is for use.
MoS2The synthesis of/CNT：
1) CNTs of 200mg surface functionalization is dispersed in 1000ml neopelexes (SDBS) solution (0.2% W/w in), it is ultrasonically treated 1h, it is spare as carbon source.
2) by 151mg sodium molybdates, 1h is to no obvious sediment for the mixing of 200mg thiocarbamides, then again will be at this solution ultrasound 30min is managed, is subsequently added into 25mlCNTs dispersion liquids and 45ml deionized waters to mixed solution, and continues to be ultrasonically treated 30min.
3) it and then by uniform solution is transferred in reaction kettle, and is heated 24 hours at 220 DEG C.By black suspension mistake It filters and is washed with deionized for several times, it is then dry in vacuum drying oven.Finally obtain MoS2/CNTs。
Above-described specific implementation mode has carried out further the purpose of the present invention, technical solution and advantageous effect It is described in detail, it should be understood that the foregoing is merely the specific implementation mode of the present invention, is not intended to limit the present invention Protection domain, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include Within protection scope of the present invention.

Claims (10)

1. a kind of preparation method of the mixed network structure of three-dimensional interconnection, which is characterized in that by carbon nanotube/detergent alkylate sulphur Sour sodium mixed solution, sodium molybdate and thiocarbamide are filtered, washed after hydro-thermal reaction, dry, and wherein carbon nanotube is surface functionalized Processing.
2. a kind of preparation method of the mixed network structure of three-dimensional interconnection according to claim 1, which is characterized in that carbon is received The surface functionalization of mitron specifically, carbon nanotube is added in sulfuric acid and nitric acid mixed solution after supersound process, take out by heating Filter, wash, be dried in vacuum overnight after obtain the carbon nanotube of surface functionalization.
3. a kind of preparation method of the mixed network structure of three-dimensional interconnection according to claim 2, which is characterized in that ultrasound Handle 10~15min.
4. a kind of preparation method of the mixed network structure of three-dimensional interconnection according to claim 2, which is characterized in that heating For 60~80 DEG C of 1~2h of oil bath heating.
5. a kind of preparation method of the mixed network structure of three-dimensional interconnection according to claim 2, which is characterized in that vacuum Dry is 50~60 DEG C.
6. a kind of preparation method of the mixed network structure of three-dimensional interconnection according to claim 1, which is characterized in that by molybdenum 1h is mixed to no obvious sediment in sour sodium, thiocarbamide, this solution is then ultrasonically treated 30~45min again, is subsequently added into CNTs Dispersion liquid and deionized water continue 30~45min of supersound process to mixed solution.
7. a kind of preparation method of the mixed network structure of three-dimensional interconnection according to claim 1, which is characterized in that carbon is received Mitron/neopelex mixed solution is that 200mg carbon nanotubes are dispersed in 1000ml neopelexes, It is ultrasonically treated 1~1.5h.
8. a kind of preparation method of the mixed network structure of three-dimensional interconnection according to claim 6, which is characterized in that carbon is received Mass ratio between mitron and sodium molybdate, thiocarbamide is 4:151:200.
9. such as the mixed network structure for the three-dimensional interconnection that claim 1-8 any one of them preparation methods obtain, it is situated between to be three-dimensional Hole Specific surface area.
10. such as the mixed network structure of claim 1-8 any one of them three-dimensional interconnections, as lithium air electrode material Using.
CN201810128640.9A 2018-02-08 2018-02-08 A kind of mixed network structure of three-dimensional interconnection, Preparation method and use Pending CN108365175A (en)

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CN114214659A (en) * 2022-01-12 2022-03-22 安徽大学 Electrocatalytic material and preparation method and application thereof
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